Purification method for erythromycin thiocyanate

A technology of erythromycin thiocyanate and a purification method, which is applied in the field of biopharmaceuticals to achieve the effects of improved fermentation level, strong process adaptability, and quality improvement

Active Publication Date: 2021-07-23
HEC PHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a purification method of erythromycin thiocyanate, which solves the deficiency of the exist

Method used

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  • Purification method for erythromycin thiocyanate
  • Purification method for erythromycin thiocyanate
  • Purification method for erythromycin thiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0030] Example 1:

[0031] Purification method of eryl matrix cytercin, the method comprising the steps of:

[0032] 1.1 Erythromycin, crude thiocyanate, distinguish

[0033] Accurately weighed erythromycin 500g according to the material than the material ratio of erythromyanate (G): butyry acetate (ml) = 1: 3.3 quantities of 1650 ml of acetate, butyl acetate is transferred into the glass After the beaker (3000ml) was opened, stirred, and erythromyanate was added, and then the temperature was increased. When the system temperature rose to 45 ° C, the stream plus a mass concentration of 5% NaOH solution, the control system pH to 10.4 until complete Dissolve, retained, phase-phase, and collect the upper laminate phase material.

[0034] 1.2 flow plus crystallization auxiliary crystallization

[0035] Formulated crystallization aid: add 40 g of solid NASCN (1.25mol equivalents) to 330mlh 2 O (20% acetate volume), at normal temperature stirred to completely dissolve, add 29 ghac (1.22...

Example Embodiment

[0043] Example 2:

[0044] Purification method of eryl matrix cytercin, the method comprising the steps of:

[0045] 2.1 sulfithromcycin dissolved, divided

[0046] Accurately weighed erythromycin 2000g, calcined by erythium thiocyanate (g) than the material ratio of stem (G): tare acetate (ml) = 1: 3.3 quantities 6600ml of acetate, butyl acetate is transferred into the glass After the dissolved tank (900 ml) was opened, stirred, erythromycin was added, and then the temperature was increased after the system temperature rose to 45 ° C, the mass concentration was 5% NaOH solution, the control system pH to 11 Completely dissolve, keep it, and phase to collect the upper laminate phase material.

[0047] 2.2 Flow Crystallization Auxiliary Crystallization

[0048] Formulated crystallization aid: add 190 g of solid NASCN (1.49mol equivalent) to 1320mlh 2O (20% acetate volume), at normal temperature stirred to completely dissolve, add 140 g HAC (1.48 mol equivalent), and stir evenly.

[...

Example Embodiment

[0056] Example 3:

[0057] Purification method of eryl matrix cytercin, the method comprising the steps of:

[0058] 3.1 Mixtymycin, sulfynin, sulphate, and phase

[0059] Accurately weighed erythromycin 36kg, steroid (G), butyl acetate (ml) = 1: 4, quantified, butyl acetate (ml) = 1: 4 quantity, deuterate 144L After the glass soluble tank (specification 250L) was opened, stirred, erythromyanate was added, and then the temperature was warmed after the system temperature rose to 40 ° C, and the stream plus the mass concentration of 10% NaOH solution, the control system pH to 10 Until completely dissolved, retained, phase-phase, and collect the upper acetate phase material.

[0060] 3.2 Flow Crystallization Auxiliary Crystallization

[0061] Preparation of crystallization aid: add 2919 g of solid NASCN (1.3mol equivalents) to 36LH 2 O (25% acetate volume), at normal temperature stirred to completely dissolve, add 1828 g HAC (1.1 mol equivalents), and stir evenly.

[0062] The above-...

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Abstract

The invention provides a purification method for erythromycin thiocyanate. The method comprises the following specific steps of S1, adding an erythromycin thiocyanate crude product into a butyl acetate solvent, performing heating to 40-50 DEG C, then adjusting the pH value to 10-11, performing heat preservation and phase separation after complete dissolution, and collecting a butyl acetate phase solution; and S2, performing heat preservation on the butyl acetate phase solution, adding methanol into the butyl acetate phase solution, adding a crystallization auxiliary agent into a system after uniformly stirring, growing crystals after material adding, then performing cooling and growing crystals again, and finally, drying the separated crystals to obtain an erythromycin thiocyanate product. According to the method, by adjusting a CH3OH consumption, impurity components such as an erythromycin B component are removed, the erythromycin component content is increased, and the provided preparation method for crystallizing the erythromycin thiocyanate under a new solvent system has characteristics of simple process, easy control and effective impurity removal.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a method for purifying erythromycin thiocyanate. Background technique [0002] Erythromycin is an antibiotic isolated from the culture medium of Saccharopolyspora ruberosa in 1952. Later, erythromycin A, B, C, D, E and other components were isolated from the fermentation broth, among which erythromycin Factor A is the main component, which has strong antibacterial activity and less toxic and side effects, while other components have weak antibacterial activity and greater toxic and side effects than A. Therefore, the current extraction and purification process of erythromycin focuses on increasing the content of the product erythromycin A component and reducing the content of the internal impurities in the erythromycin B component. Erythromycin thiocyanate is an intermediate of the macrolide antibiotic erythromycin. This product is generally used as a pharmaceutical intermediat...

Claims

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Application Information

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IPC IPC(8): C07H1/06C07H17/08
CPCC07H1/06C07H17/08
Inventor 邹兵商清海邓肇政熊辉
Owner HEC PHARM
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